Abstract

Ceria hexaniobate nanopeapods have been prepared and their formation and assembly studied. Various sized ceria nanocubes (5 to 40 nm) were synthesized via a solvothermal approach with oleic acid and oleylamine capping agents. Utilizing a second solvothermal treatment, the nanoparticles were then captured within scrolling hexaniobate nanosheets to produce ceria@hexaniobate nanopeapods. In some instances, peapods were partially filled with ceria so that in a subsequent step, open sites could be filled with Au nanoparticles via in situ growth methods leading to arrangements of gold and ceria NPs within nanoscrolls. Studies on nanoparticle assembly and encapsulation were also carried out. Size‐selective preassembly of nanoparticles on hexaniobate nanosheet surfaces is observed prior to scrolling, after which smaller ceria NPs (ca. ≤ 10 nm) are efficiently captured inside scrolled nanosheets. Improved understanding and control of this behavior is important for further development of more intricate multicomponent particles assemblies and formations within varieties of tubular structures with different morphological and structural features.

The use of microwave irradiation for the synthesis of inorganic nanomaterials has recently become a widespread area of research that continues to expand in scope and specialization. The growing demand for nanoscale materials with composition and morphology tailored to specific applications requires the development of facile, repeatable, and scalable synthetic routes that offer a high degree of control over the reaction environment. Microwave irradiation provides unique advantages for developing such routes through its direct interaction with active reaction species, which promotes homogeneous heat distribution, increased reaction rates, greater product quality and yield, and use of mild reaction conditions. Many catalytic nanomaterials such as noble metal nanoparticles and intricate nanocomposites have very limited synthetic routes due to their extreme temperature sensitivity and difficulty achieving homogeneous growth. This work presents recent advances in the use of MW irradiation methods to produce high-quality nanoscale composites with controlled size, morphology, and architecture.